CN102719858B - Preparation method of dendritic nano silver - Google Patents
Preparation method of dendritic nano silver Download PDFInfo
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- CN102719858B CN102719858B CN201210178847.XA CN201210178847A CN102719858B CN 102719858 B CN102719858 B CN 102719858B CN 201210178847 A CN201210178847 A CN 201210178847A CN 102719858 B CN102719858 B CN 102719858B
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Abstract
The invention discloses a preparation method of dendritic nano silver. The preparation of dendritic nano silver is performed in a microorganism electrochemical tank. The microorganism electrochemical tank comprises a biological anode, a diaphragm, a cathode, an anolyte and a catholyte, the anolyte contains organic matters capable of being biologically oxidized and degraded, the catholyte contains free or complex silver ion, the microorganism on the anode oxidizes the organic matters in the anolyte to release electrons, and the electrons are transferred to the cathode by an external circuit so as to deposit the silver ion in the catholyte on the cathode in the form of dendritic nano silver. The method for preparing dendritic nano silver is low in cost, environment-friendly in process and is easy for industrial production operation.
Description
Technical field
The invention belongs to the general field of material, nanometer technology and wastewater treatment, be specifically related to a kind of preparation method of dendritic nano-silver.
Background technology:
The precious metal material of nanoscale gets more and more people's extensive concerning due to its excellent catalytic performance, electric property, magnetic performance and optical property etc. in recent years.Different shape and structure such as graininess, wire, bar-shaped, sheet, irregular metal nanoparticle are synthesized in succession.Dendritic nano-silver obtains large quantity research because of its special structure and potential use.People prepare the dendritic nano-silver of different shape respectively by methods such as electrochemical deposition, electronation, UV irradiation.Often need complexity, expensive organic chemical reagent as reducing agent, stabilizing agent and complexing agent etc. in these methods, and these chemical reagent and silver ion mix and cause the separation and purification cost of prepared dendritic nano-silver to improve.
Summary of the invention
The object of the present invention is to provide a kind of preparation method of easy, cheap dendritic nano-silver.The method, without the need to the organic chemical reagent of costliness, does not also consume electric energy, and the dendritic nano-silver of preparation is deposited directly on electrode.
For achieving the above object, the technical solution used in the present invention is:
1) first, by barrier film, microorganism electrochemical pond is divided into cathode chamber and anode chamber;
2) secondly, the aqueous solution of the silver ion of 0.005-0.2mol/L is placed in cathode chamber, then the negative electrode made by material with carbon element is placed in cathode chamber;
3) then, the aqueous solution of the biodegradable organic containing 0.01mmol/L-1mol/L or sanitary sewage are placed in anode chamber, then the anode be made up of electrogenesis microorganism and substrate is placed in anode chamber;
4) last, anode is connected by external load R with negative electrode, by size and the discharge time of regulating load, controls silver ion reduction and produce the speed of dendritic nano-silver and the size of dendritic nano-silver.
Described barrier film is cation-exchange membrane, anion-exchange membrane or Bipolar Membrane.
The aqueous solution of described silver ion is the aqueous solution containing free silver ions or complex silver ion.
Described negative electrode adopts graphite, vitreous carbon, carbon black or charcoal cloth to make.
The aqueous solution of described biodegradable organic is acetate, glucose, starch, ammonia nitrogen or cellulose.
The electrogenesis microorganism of described anode is tamed by anaerobic grain sludge and obtains.
The substrate of described anode is charcoal felt, charcoal cloth, carbon paper or graphite are made.
Described external load R adopts power consuming device pure resistance or bulb.
Adopt preparation method of the present invention very conveniently can produce dendritic nano-silver at an easy rate, the preparation for this nano silver material provides a kind of new technology, for the extensive use of dendritic nano-silver lays the foundation.
Accompanying drawing explanation
Fig. 1 is microorganism electrochemical pool structure schematic diagram of the present invention;
Fig. 2 is the lower multiple scanning electron microscope (SEM) photograph of dendritic nano-silver prepared by the present invention;
Fig. 3 is the scanning electron microscope (SEM) photograph of the higher multiple of dendritic nano-silver prepared by the present invention;
Fig. 4 is the XRD spectra of dendritic nano-silver prepared by the present invention.
Detailed description of the invention
Below in conjunction with accompanying drawing, the present invention is described in further detail.
Embodiment 1:
See Fig. 1,1) first, by cation-exchange membrane 2, microorganism electrochemical pond 1 is divided into cathode chamber 3 and anode chamber 4;
2) secondly, the aqueous solution containing free silver ions of 0.005mol/L is placed in cathode chamber 3, then the negative electrode 5 made by graphite is placed in cathode chamber 3;
3) then, be placed in containing the acetate aqueous solution of 0.01mmol/L in anode chamber 4, then be placed in anode chamber 4 by being tamed the anode 6 that substrate that the electrogenesis microorganism that obtains becomes with charcoal felt forms by anaerobic grain sludge;
4) last, anode 6 is connected by external load R with negative electrode 5, by size and the discharge time of regulating load, controls silver ion reduction and produce the speed of dendritic nano-silver and the size of dendritic nano-silver.
Embodiment 2:
1) first, by anion-exchange membrane 2, microorganism electrochemical pond 1 is divided into cathode chamber 3 and anode chamber 4;
2) secondly, the aqueous solution containing complex silver ion of 0.001mol/L is placed in cathode chamber 3, then the negative electrode 5 made by vitreous carbon is placed in cathode chamber 3;
3) then, the aqueous solution of glucose containing 0.5mmol/L is placed in anode chamber 4, then is placed in anode chamber 4 by being tamed the anode 6 that substrate that the electrogenesis microorganism that obtains and charcoal cloth makes forms by anaerobic grain sludge;
4) last, anode 6 is connected by external load R with negative electrode 5, by size and the discharge time of regulating load, controls silver ion reduction and produce the speed of dendritic nano-silver and the size of dendritic nano-silver.
Embodiment 3:
1) first, by Bipolar Membrane 2, microorganism electrochemical pond 1 is divided into cathode chamber 3 and anode chamber 4;
2) secondly, the aqueous solution containing free silver ions of 0.05mol/L is placed in cathode chamber 3, then the negative electrode 5 made by carbon black is placed in cathode chamber 3;
3) then, be placed in containing the amidin of 5mmol/L in anode chamber 4, then be placed in anode chamber 4 by being tamed the anode 6 that substrate that the electrogenesis microorganism that obtains and carbon paper make forms by anaerobic grain sludge;
4) last, anode 6 is connected by external load R with negative electrode 5, by size and the discharge time of regulating load, controls silver ion reduction and produce the speed of dendritic nano-silver and the size of dendritic nano-silver.
Embodiment 4:
1) first, by cation-exchange membrane 2, microorganism electrochemical pond 1 is divided into cathode chamber 3 and anode chamber 4;
2) secondly, the aqueous solution containing complex silver ion of 0.1mol/L is placed in cathode chamber 3, then the negative electrode 5 made by charcoal cloth is placed in cathode chamber 3;
3) then, be placed in containing the ammonia nitrogen aqueous solution of 0.5mol/L in anode chamber 4, then be placed in anode chamber 4 by being tamed the anode 6 that substrate that the electrogenesis microorganism that obtains and graphite makes forms by anaerobic grain sludge;
4) last, anode 6 is connected by external load R with negative electrode 5, by size and the discharge time of regulating load, controls silver ion reduction and produce the speed of dendritic nano-silver and the size of dendritic nano-silver.
Embodiment 5:
1) first, by anion-exchange membrane 2, microorganism electrochemical pond 1 is divided into cathode chamber 3 and anode chamber 4;
2) secondly, the aqueous solution containing free silver ions of 0.15mol/L is placed in cathode chamber 3, then the negative electrode 5 made by graphite is placed in cathode chamber 3;
3) then, be placed in containing the cellulosic aqueous solution of 1mol/L in anode chamber 4, then be placed in anode chamber 4 by being tamed the anode 6 that substrate that the electrogenesis microorganism that obtains becomes with charcoal felt forms by anaerobic grain sludge;
4) last, anode 6 is connected by external load R with negative electrode 5, by size and the discharge time of regulating load, controls silver ion reduction and produce the speed of dendritic nano-silver and the size of dendritic nano-silver.
Embodiment 6:
1) first, by Bipolar Membrane 2, microorganism electrochemical pond 1 is divided into cathode chamber 3 and anode chamber 4;
2) secondly, the aqueous solution containing complex silver ion of 0.2mol/L is placed in cathode chamber 3, then the negative electrode 5 made by charcoal cloth is placed in cathode chamber 3;
3) then, sanitary sewage is placed in anode chamber 4, then is placed in anode chamber 4 by being tamed the anode 6 that substrate that the electrogenesis microorganism that obtains and graphite makes forms by anaerobic grain sludge;
4) last, anode 6 is connected by external load R with negative electrode 5, by size and the discharge time of regulating load, controls silver ion reduction and produce the speed of dendritic nano-silver and the size of dendritic nano-silver.
Class anode substrate of the present invention can make electrogenesis microbial adhesion and by microbiological oxidation organic matter produce electro transfer to external circuit.Barrier film is cation-exchange membrane or anion-exchange membrane or Bipolar Membrane, the silver ion diffusion of cathode chamber can be stoped to poison anode microorganism to anode, also anode chamber's organic matter can be stoped to be diffused into the dendritic nano-silver of cathode contamination generation, but can conducting hydrogen ion or hydroxide ion.
In mentioned microorganism electrochemical cell, microorganism anode is connected by external load R with negative electrode, external load comprises the device of the power consumption such as pure resistance, miniature bulb, by regulating different loads and discharge time, load can regulate between 50 ohm to 10000 ohm, the discharge depositing time in 1 little adjustment between 10 days, can control silver ion reduction and produce the speed of dendritic nano-silver and the size of dendritic nano-silver.
By Fig. 2,3 can find out dendritic nano-silver prepared by the present invention, and deposited material is dendritic nanostructures, branch trunk is about 20-40um, branch diameter 200-500nm, and branch and trunk are in about 45 degree of angles, branch is about less than 1um to several um, branch diameter and trunk similar diameters.
Can find out that the material of the dendritic structure be deposited on graphite electrode is Nano Silver really by the X ray diffracting spectrum of Fig. 4.The crystal face Ag(111 of Nano Silver), Ag(200), Ag(220), Ag(311) be labeled on XRD spectra, and the signal of substrate graphite is at 25.8 and 54 degree of places, has also been labeled on XRD spectra.
Claims (7)
1. a preparation method for dendritic nano-silver, is characterized in that:
1) first, by barrier film (2), microorganism electrochemical pond (1) is divided into cathode chamber (3) and anode chamber (4);
2) secondly, the aqueous solution of the silver ion of 0.005-0.2mol/L is placed in cathode chamber (3), then the negative electrode (5) made by material with carbon element is placed in cathode chamber (3);
3) then, the aqueous solution of the biodegradable organic containing 0.01mmol/L-1mol/L or sanitary sewage are placed in anode chamber (4), then the anode be made up of electrogenesis microorganism and substrate (6) is placed in anode chamber (4); The electrogenesis microorganism of described anode is tamed by anaerobic grain sludge and obtains;
4) last, anode (6) is connected by external load R with negative electrode (5), by size and the discharge time of regulating load, controls silver ion reduction and produce the speed of dendritic nano-silver and the size of dendritic nano-silver.
2. the preparation method of dendritic nano-silver according to claim 1, is characterized in that: described barrier film (2) is cation-exchange membrane, anion-exchange membrane or Bipolar Membrane.
3. the preparation method of dendritic nano-silver according to claim 1, is characterized in that: the aqueous solution of described silver ion is the aqueous solution containing free silver ions or complex silver ion.
4. the preparation method of dendritic nano-silver according to claim 1, is characterized in that: described negative electrode adopts graphite, vitreous carbon, carbon black or charcoal cloth to make.
5. the preparation method of dendritic nano-silver according to claim 1, is characterized in that: described biodegradable organic is acetate, glucose, starch, ammonia nitrogen or cellulose.
6. the preparation method of dendritic nano-silver according to claim 1, is characterized in that: the substrate of described anode is charcoal felt, charcoal cloth, carbon paper or graphite are made.
7. the preparation method of dendritic nano-silver according to claim 1, is characterized in that: described external load R adopts power consuming device pure resistance or bulb.
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| CN105908220B (en) * | 2016-05-06 | 2018-03-30 | 上海应用技术学院 | A kind of method that liquid electrodeposition prepares micro-nano silver dendrite |
| CN109234768A (en) * | 2018-11-09 | 2019-01-18 | 广东顺德西安交通大学研究院 | A kind of electrochemical appliance preparing nano-Ag particles and method |
| CN109208020A (en) * | 2018-11-09 | 2019-01-15 | 广东顺德西安交通大学研究院 | A kind of electrochemical appliance and method synthesizing nano cuprous oxide |
| CN110387555B (en) * | 2019-07-17 | 2020-05-22 | 湖北省农业科学院农产品加工与核农技术研究所 | Method for preparing plant starch glucan by weak electrolysis method |
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Effective date of registration: 20170605 Address after: 523085 Guangdong city of Dongguan province water Road No. 96 branch of the international information industry park 20 Patentee after: Guangdong Vojssen environmental protection Polytron Technologies Inc Address before: 710049 Xianning West Road, Shaanxi, China, No. 28, No. Patentee before: Xi'an Jiaotong University |